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Preparation method of 1T-phase molybdenum disulfide

A molybdenum disulfide, molybdenum source technology, applied in the direction of molybdenum sulfide and other directions, can solve the problem of inability to prepare 1T phase molybdenum disulfide by one-pot reaction, and achieve the effects of high production efficiency and safe preparation process

Active Publication Date: 2017-05-31
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem that the existing technology cannot prepare 1T phase molybdenum disulfide by one-pot reaction, the present invention provides a preparation method for one-step hydrothermal synthesis of 1T phase molybdenum disulfide, which aims to simplify the preparation process of 1T phase molybdenum disulfide and improve production Efficiency and manufacturing safety

Method used

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  • Preparation method of 1T-phase molybdenum disulfide
  • Preparation method of 1T-phase molybdenum disulfide
  • Preparation method of 1T-phase molybdenum disulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Place 0.88g ammonium molybdate, 0.94g thioacetamide and 1.98g ammonium bicarbonate in 40ml distilled water, stir with a magnetic stirrer for 30 minutes until the solution is colorless and transparent, pour it into the reactor and seal it, then Heat to 200°C and keep it warm for 13 hours. After cooling to room temperature, wash the product with distilled water and absolute ethanol, and dry it in a constant temperature drying oven at 60°C for 12 hours to obtain a black powder product. like figure 1 , the existence of 1T molybdenum disulfide can be preliminarily obtained through Raman spectroscopy, where the j 1 , j 2 and j 3 The characteristic peak represents the 1T phase molybdenum disulfide. pass figure 2 , XPS analysis further confirmed the presence of 1T phase molybdenum disulfide in the obtained molybdenum disulfide, and the proportion of 1T phase was greater than that of 2H phase. like image 3 , the existence of 1T phase molybdenum disulfide can be directly ...

Embodiment 2

[0046] Place 0.88g ammonium molybdate, 0.94g thioacetamide and 1.98g ammonium bicarbonate in 40ml distilled water, stir with a magnetic stirrer for 30 minutes until the solution is colorless and transparent, pour it into the reactor and seal it, then Heat to 180°C and keep it warm for 13 hours. After it is cooled to room temperature, wash the product with distilled water and absolute ethanol, and dry it in a constant temperature drying oven at 60°C for 12 hours to obtain 1T phase molybdenum disulfide. Among the hydrothermal products, the 1T phase product content is 53.7%.

Embodiment 3

[0048] Place 0.88g ammonium molybdate, 0.94g thioacetamide and 1.98g ammonium bicarbonate in 40ml distilled water, stir with a magnetic stirrer for 30 minutes until the solution is colorless and transparent, pour it into the reactor and seal it, then Heat to 160°C and keep it warm for 13 hours. After cooling to room temperature, wash the product with distilled water and absolute ethanol, and dry it in a constant temperature drying oven at 60°C for 12 hours to obtain 1T phase molybdenum disulfide. In the hydrothermal product, the 1T phase product content is 50.3%.

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Abstract

The invention discloses a preparation method of 1T-phase molybdenum disulfide. The preparation method comprises the step of performing a hydrothermal reaction on an aqueous solution comprising a molybdenum source, a sulfur source and an ammonia source at 160-220 DEG C to prepare the 1T-phase molybdenum disulfide. The ammonia source is organic quaternary ammonium salt and / or inorganic ammonia salt. According to the preparation method disclosed by the invention, under the synergistic effect of the ammonia source and the hydrothermal reaction temperature, the 1T-phase molybdenum disulfide can be prepared through a one-pot reaction. The preparation method is simple, high in production efficiency and safe in preparation process.

Description

technical field [0001] The invention relates to a preparation method of 1T phase molybdenum disulfide, which belongs to the field of preparation of inorganic material molybdenum disulfide. Background technique [0002] As an important two-dimensional layered nanomaterial, molybdenum disulfide is widely used in friction lubrication, catalytic refining, Hydrogen storage materials, photoelectric hydrogen production catalysts and many other fields. In general, molybdenum disulfide has a variety of crystal structures, the most common of which are 1T, 2H, and 3R crystal structures. Among them, 2H and 3R phase molybdenum disulfide are semiconductors, while 1T phase molybdenum disulfide is metallic. In addition, 1T phase molybdenum disulfide has outstanding performance in the field of photoelectric hydrogen production catalysis. Ordinary 2H phase molybdenum disulfide has poor electrical conductivity, and its hydrogen evolution catalytic active sites are mainly distributed on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06
CPCC01G39/06C01P2002/82C01P2002/85C01P2004/04
Inventor 吴壮志王德志张祥勇
Owner CENT SOUTH UNIV
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